Process for making shaped, rapidly and easily soluble mixtures of soaps and persalts



252. COM

POSITIONS,

Patented Dec. 19, 1933 UNITED STATES PROCESS FOR. MAKING SHAPED, RAPIDLY AND EASILY SOLUBLE MIXTURES SOAPS AND PERSALTS Adolf Welter, Krefeld, Germany No Drawing. Application June 24, 1931, Serial No. 546,661, and in Germany May 17, 1927 3 Claims.

A process has already been proposed by the applicant for making high-percentage, waterfree and stable, non-efilorescing, powdered or shaped soaps with or without addition of fatdissolving media, which consists in mixing fatty acid, which has been split up as highly as possible or distilled, with or without addition of fat solvents, with a weight of anhydrous calcined soda, or of soda having only a small moisture content, which slightly exceeds double the quantity of that necessary for complete saponification, said mixing being carried out at a low temperature which, however, still permits of intimate admixture being effected, after which the mass, completely saponified owing to spontane ous heating, is, after cooling, ground to a fine powder in the known manner and the resulting powder pressed into pieces, or the still incompletely solidified mass is, before it has become brittle, shaped into solid piping by mechanical or hydraulic presses in an operative process, and then allowed to cool.

The applicant has now ascertained that, using this production process, shapable, rapidly and readily-soluble mixtures of soaps and persalts can be made if the persalt is already admixed in the course of the saponification process. Preferably one starts from fats which are as pure as possible, more particularly from those having a not too high iodine number. Of course, other electrolytes besides the persalts can be added during the saponification reaction, such as, for example, sodium tri-phosphate, sodium pyrophosphate, sodium bicarbonate, borax or the like, chiefly in those cases in which the fatty acid content is to be diminished.

A mixture prepared in this way contains the persalt in an extremely stable form. This stability of the persalts may be further increased by adding for the protection thereof to the mass to be worked up a known addition of hydrocarbons which are insensitive towards oxygen.

By means of this process completely waterfree soaps are obtained, which already as a result of this freedom from water ensure that the persalts, which are very sensitive towards water, do not show any such rapid loss of oxygen. The shaping may be carried out either by rolling to platelets between highly polished rollers, or by rolling on roller mills and scraping off the thin soap film by means of suitable knives or needles, or finally by pressing the soap mixture to very fine threads through smallest nozzles. In this way shaped soap of fine appearance is obtained in the form of platelets, wool, filaments, or tiny needles (which latter are formed by breaking the fine filaments). On account of their freedom from water these products show not only a very high stability but they are very rapidly and readily soluble as well, as a result of which it is ensured as much as possible that the textile material is not impaired. If the mixture of soap and persalt should be too brittle for shaping, then this diificulty may bereadily overcome by replacing a part of the calcined soda by a 5 corresponding quantity of potash or potassium carbonate. Of course, additions of protective colloids, such as, for example, of water-glass or substance having an anti-catalytic effect is also readily possible. It has now been found that the soaps prepared in this way from fatty acids and soda are, after admixture with persalts and shaping, comparatively very stable as regards oxygen content and in any case show a higher stability than when grain soaps are used made from the same fatty acids and dried, although still containing water. This stability may be very considerably enhanced if hydrocarbons insensitive towards oxygen are added in the known manner at the same time in the course of the process of producing soap from fatty acids and soda, it having been found that these additions just here, not only offer protection against the moisture which promotes decomposition, but they also act anti-catalytically and further slow down and disseminate the heat evolution which proceeds during all the operations here taking place, so that no temperature so high as to be harmful to the perborate, is reached.

Examples (1) 100 kg. of a mixture comprised of 70% coconut oil fatty acid which has been highly split, and 30% of tallow oil fatty acid or hard oil fatty acid, likewise highly split, are saponified with 30 kg. of calcined soda and 5 kg. of potash or potassium carbonate in an aluminium vessel at 35 C. Just before the reaction mass goes over into a viscous solid state 12-13 kg. of sodium perborate are added. Before the mass becomes completely cold and brittle it is rolled out between highly polished steel or stone rollers to thin platelets or fine thin strips.

(2) 100 kg. of a mixture comprised of highly split hardened palm-kernel oil fatty acid and hardened groundnut oil fatty acid are saponified as stated in Example 1 with 33 kg. of calcined soda and 10 kg. of potash or potassium carbonate. Just before the mass becomes solid 14 11 kg. of sodium perborate are added which has preferably been worked up to a dough with about the same quantity of water-glass. After the saponiflcation produced by spontaneous heating has almost reached completion, the mass is shaped in the form of strips on roller mills, is then pressed to solid-piping from which fine platelets are scraped oil by means of rotating knives after it has cooled and become brittle.

(3) 100 kg. of a highly split fatty acid consisting of 50% coconut oil fatty acid and 50% of tallow fatty acid are saponified at 35", as stated in Example 1, with 33 kg. of calcined soda and 18 kg. of sodium perborate in presence of 20-22 kg. of a pure benzine boiling between 180 and 200. The product is then rolled out on a roller mill, the soap being removed from the rollers in the form of a fine soap wool by means of suitable fine needles.

(4) 100 kg. of liquid distilled ground nut oil fatty acid are thoroughly stirred up with 44 kg. of calcined soda at a moderate heat. After about half an hour the mass is completely uniform and somewhat stiff. 15 kg. of sodium perborate are now added. The mass then becomes so stitf that it can be thrown out without any further preliminary. After a few hours the mixture becomes so brittle that it can be ground to a powder. This powder consists only of water-free soap, sodium bicarbonate, and sodium perborate having a fatty acid content of about 62% and an active oxygen content of about 0.98%. Excess of soda is not present, but merely bicarbonate. Also the oxygen content does not deteriorate after very long storage.

(5) The proceedure is as described in Example 4, but 100 kg. of the powder obtained therein is mixed in addition with 55 kg. of sodium trlphosphate and in this way a thoroughly stable product is likewise obtained containing about 41% fatty acid and 0.6% of active oxygen. The mixture dissolves at 40 in distilled water to give a perfectly clear solution and it exhibits particularly good lather and cleansing properties.

(6) 100 kg. of a distilled fatty acid, in admixture with 20-22 kg. of benzine or xylene or hydrogenated hydrocarbons are saponified with 34 kg. of calcined soda, as described in Example 1; at the end of the saponification reaction 18 kg. of sodium perborate are added.

The soap is rolled once through a roller mill and the strips obtained are pressed through flne spinnerets. Should the soap mass be too brittle or too solid for this pressing operation, some liquid grain soap is added to it in a mixing machine. The necessary plasticity is then reached in a short time. In this way highly lustrous white filaments, looking almost the same as artificial silk, are obtained which are already so completely saponified after a few hours that they readily and rapidly dissolve and give a perfectly clear solution in distilled water and, moreover, they show great stability as regards oxygen content.

It has already been proposed to admix perborate with a ready boiled soap of definite water content, hydrocarbons being added as well if desired, and then to roll the mixture in order to flake it. In this prior process, therefore, the perborate was added to ready manufactured soap containing water; according to applicants invention, however, this addition is effected during the saponification process itself and the soap is practically free from water. Substantial advantages are obtained hereby. Since a start is made, not with boiled soap but with a soap made without boiling, according to the manner described, the saponiflcation can be commenced at a very low temperature, for example, at 35 0., without the temperature rise which results thereby attaining 100 C., so that a temperature which is injurious for the stability of the persalt to be added is not reached. The persalt can be stirred in at the low temperature, as a result of which much better admixture is produced, quite apart from the fact that a boiler is dispensed with and all the disadvantages attending the use of the same are avoided. Further, the fact that a water-free product is obtained owing to the nature of the saponification process used renders decomposition of the persalts by water completely out of the question and ensures for them a degree of stability which has not been attained hitherto.

What I claim is:

1. A process for making a substantially anhydrous persalt soap which is readily soluble in water, consisting in mixing about 100 parts of highly split, saponifiable and saturated fatty acids of the non-drying oils with 44 parts of calcined soda, the spontaneous heat of reaction causing the saponiflcation, stirring the thus saponified mass until it becomes still, incorporating 15 parts of sodium perborate into said saponified mass before the reaction mass goes over into solid state, and lastly forming the soap mass into desired shape before the mass is cold and brittle; all parts measured by weight.

2. A process for making a substantially anhydrous persalt soap which is readily soluble in water, consisting in mixing about 100 parts of highly split, saponifiable and saturated fatty acids of the non-drying oils with 44 parts of calcined soda, the spontaneous heat of reaction causing the saponiflcation, stirring the thus saponified mass until it becomes stiff, incorporating 55 parts of sodium triphosphate, incorporating 15 parts of sodium perborate into said saponified mass before the reaction mass goes over into solid state, and lastly forming the soap mass into desired shape before the mass is cold and brittle; all parts measured by weight.

3. A process for making a substantially anhydrous persalt soap which is readily soluble in water, consisting in mixing about 100 parts of highly split, saponifiable and saturated fatty acids of the non-drying oils witht 44 parts of calcined soda, the spontaneous heat of reaction causing the saponification, stirring the thus saponified mass until it becomes stifl, incorporating 21 parts of liquid hydrocarbon, incorporating 15 parts of sodium perborate into said saponified mass before the reaction mass goes over into solid state, and lastly, forming the soap mass into desired shape before the mass is cold and brittle; all parts measured by weight.

ADOLF WELTER. 

